CN1683382A - Process for extracting phlorhizin from bark, root, branch and leaf of rosaceous plant and juice pressing waste material - Google Patents
Process for extracting phlorhizin from bark, root, branch and leaf of rosaceous plant and juice pressing waste material Download PDFInfo
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- CN1683382A CN1683382A CN 200510016291 CN200510016291A CN1683382A CN 1683382 A CN1683382 A CN 1683382A CN 200510016291 CN200510016291 CN 200510016291 CN 200510016291 A CN200510016291 A CN 200510016291A CN 1683382 A CN1683382 A CN 1683382A
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Abstract
The phlorhizin extracting process includes the following steps: 1) soaking material in alcohol, heating to boil, filtering and concentrating the filtrate while recovering alcohol; 2) adsorbing the filtrate in macroporous resin, gradient eluting with alcohol solution of 20 %, 40%, 60 % and 80 % concentration successively, sectional collecting effluent, concentrating, extracting with chloroform, eliminating chloroform layer, re-concentrating to specific density of 1-1.08, and separating crystal at 0-4 deg.c. The present invention has cheap material, simple extracting process, low power consumption and less harmful solvent residue, and is meet the requirement for use in medicine and food.
Description
Technical field
The present invention relates to a kind of extraction process of natural phant effective ingredient, particularly relating to a kind of bark with rosaceous plant, root, branches and leaves and the waste material of squeezing the juice is raw material, extracts the technology of phlorizin.
Background technology
Phlorizin belongs to the plant polyphenol compounds.External more for the research of phlorizin relevant physiological function.Phlorizin can activate the cellular protein expression kinases, and the unordered hyperplasia of pair cell has restraining effect, is a kind of antimutagenic factor, can be used for the assisting therapy of skin liver cancer and other tumours.Phlorizin content dependency (Shinohara 1998) studies show that phlorizin can effectively slow down the proliferate of colon cancer cell and liver neoplasm cell; Extremely strong antioxygen is arranged, to greasy anti-oxidant concentration between 10-30ppm; Phlorizin has remarkable step-down, effect for reducing fat, and being described as by the people is " natural depressor ", particularly suitable for hypertensive patient or hyperlipidemia patient; The phlorizin external application can stop carbohydrate content to enter epidermic cell, thereby suppresses the excessive secretion of cutaneous gland, the vigorous type acne of treatment secretion; Phlorizin can suppress the melanocyte activity, and various skin splashs are had desalination effect etc.(1998) such as Kanda of Japan confirm that " phlorizin " that extract can effectively suppress the free and hyaluronic activity of histamine from immature green apple, play antianaphylactic effect, in addition, anti-dental caries, reducing cholesterol and the effect of preventing and treating cardiovascular disorder all have report.Phlorizin since its unique physiologically active and health-care effect in recent years in America and Europe's fields such as foodstuffs industry, cosmetic industry and medicine industry; A kind of situation of selling well healthcare products have been become.
Summary of the invention
The purpose of this invention is to provide the technology of extracting phlorizin a kind of skin, root, branches and leaves and the waste material of squeezing the juice from rosaceous plant.
Technical scheme of the present invention is summarized as follows:
Extract the technology of phlorizin a kind of skin, root, branches and leaves and the waste material of squeezing the juice, comprise the steps: from rosaceous plant
(1) raw material being added 4-10 percent by volume doubly is the ethanol of 30%-70%, soaks 1-3 hour, is heated to and boils, and keeps little and boils 2-3 hour, filters; Residue is that the ethanol of 30%-70% is heated to and boils with 2-8 percent by volume doubly, keeps little and boiled 2-3 hour, this process 1 to 3 once, collect filtered liquid, concentrate and reclaim ethanol to filtered liquid and do not have alcohol and distinguish the flavor of; (2) filtered liquid is through macroporous resin adsorption, and the ethanol gradient elution with 20%, 40%, 60%, 80% with the effluent liquid Fractional Collections, concentrates, and uses chloroform extraction, abandons chloroform layer, and reconcentration to proportion is 1-1.08, separates out crystallization for 0-4 ℃.
Described crystallization is filtered with the ethyl alcohol recrystallization of 40%-60%, and drying gets crystallization shape powder, to reach the purpose of purification.
Described rosaceous plant is apple or pears or peach or cherry or other rosaceous edible plants.
The amount of alcohol of described immersion raw material preferably raw material 6-8 doubly.
Advantage of the present invention is:
Can adopt skin, root and the branches and leaves of cheap rosaceous plant, even extract phlorizin from depleted is squeezed the juice waste material, raw material is easy to get, and turns waste into wealth.Extraction process is simple, and it is low to consume energy.
In technological process, mainly adopt extraction using alcohol, make the less residue of hazardous solvent in the raw material, meet the requirement of country food and medicine.
Description of drawings
Fig. 1 is the collection of illustrative plates of the HPLC of the raw material of production phlorizin;
Fig. 2 is the collection of illustrative plates of the HPLC of phlorizin 50% sample;
Fig. 3 is the collection of illustrative plates of the HPLC of phlorizin 98% sample;
Fig. 4 is the collection of illustrative plates of the HPLC of phlorizin standard substance.
Embodiment
The present invention is further illustrated below in conjunction with specific embodiment.
Embodiment 1
Extract the technology of phlorizin a kind of skin, root, branches and leaves and the waste material of squeezing the juice, comprise the steps: from rosaceous plant
(1) is that 3% apple squeezes the juice that to add 8 times percent by volume be 50% ethanol to waste material with water content, soaked 3 hours, be heated to and boil, keep little and boiled 2 hours, filtration; Residue is that 50% ethanol is heated to and boils with 6 times percent by volume, keeps little and boils 2 hours, and this process 2 times is collected filtered liquid, concentrates to reclaim ethanol to filtered liquid and do not have the alcohol flavor; (2) filtered liquid is through macroporous resin T2401 absorption, and the ethanol gradient elution with 20%, 40%, 60%, 80% with the effluent liquid Fractional Collections, concentrates, and uses chloroform extraction, abandons chloroform layer, and reconcentration to proportion is 1.08, separates out crystallization for 0-4 ℃.
Embodiment 2
Extract the technology of phlorizin a kind of skin, root, branches and leaves and the waste material of squeezing the juice, comprise the steps: from rosaceous plant
(1) is that 1% apple squeezes the juice that to add 7 times percent by volume be 70% ethanol to waste material with water content, soaked 2 hours, be heated to and boil, keep little and boiled 3 hours, filtration; Residue is that 70% ethanol is heated to and boils with 5 times percent by volume, keeps little and boils 2 hours, and this process 3 times is collected filtered liquid, concentrates to reclaim ethanol to filtered liquid and do not have the alcohol flavor; (2) filtered liquid is through macroporous resin adsorption, and the ethanol gradient elution with 20%, 40%, 60%, 80% with the effluent liquid Fractional Collections, concentrates, and uses chloroform extraction, abandons chloroform layer, and reconcentration to proportion is 1.08, separates out crystallization for 0-4 ℃.
Crystallization with 50% ethyl alcohol recrystallization, is filtered, drying, crystallization shape powder, to reach the purpose of purification.
Embodiment 3
Extract the technology of phlorizin a kind of skin, root, branches and leaves and the waste material of squeezing the juice, comprise the steps: from rosaceous plant
(1) is that 3% pears squeeze the juice that to add 4 times percent by volume be 30% ethanol to waste material with water content, soaked 1 hour, be heated to and boil, keep little and boiled 3 hours, filtration; Residue is that 30% ethanol is heated to and boils with 8 times percent by volume, keeps little and boils 2 hours, collects filtered liquid, concentrates to reclaim ethanol to filtered liquid and do not have the alcohol flavor; (2) filtered liquid is through macroporous resin adsorption, and the ethanol gradient elution with 20%, 40%, 60%, 80% with the effluent liquid Fractional Collections, concentrates, and uses chloroform extraction, abandons chloroform layer, and reconcentration to proportion is 1, separates out crystallization for 0-4 ℃.
Crystallization with 40% ethyl alcohol recrystallization, is filtered, drying, crystallization shape powder, to reach the purpose of purification.
Embodiment 4
Extract the technology of phlorizin a kind of skin, root, branches and leaves and the waste material of squeezing the juice, comprise the steps: from rosaceous plant
(1) is that 3% peach squeezes the juice that to add 10 times percent by volume be 60% ethanol to waste material with water content, soaked 1 hour, be heated to and boil, keep little and boiled 3 hours, filtration; Residue is that 30% ethanol is heated to and boils with 2 times percent by volume, keeps little and boils 3 hours, collects filtered liquid, concentrates to reclaim ethanol to filtered liquid and do not have the alcohol flavor; (2) filtered liquid is through macroporous resin adsorption, and the ethanol gradient elution with 20%, 40%, 60%, 80% with the effluent liquid Fractional Collections, concentrates, and uses chloroform extraction, abandons chloroform layer, and reconcentration to proportion is 1, separates out crystallization for 0-4 ℃.
Crystallization with 60% ethyl alcohol recrystallization, is filtered, drying, crystallization shape powder, to reach the purpose of purification.
Embodiment 5
Extract the technology of phlorizin a kind of skin, root, branches and leaves and the waste material of squeezing the juice from rosaceous plant, comprise the steps: that (1) is that 2% cherry squeezes the juice that to add 6 times percent by volume be 30% ethanol to waste material with water content, soaked 2 hours, be heated to and boil, keep little and boiled 2 hours, filter; Residue is that 30% ethanol is heated to and boils with 2 times percent by volume, keeps little and boils 3 hours, collects filtered liquid, concentrates to reclaim ethanol to filtered liquid and do not have the alcohol flavor; (2) filtered liquid is through macroporous resin adsorption, and the ethanol gradient elution with 20%, 40%, 60%, 80% with the effluent liquid Fractional Collections, concentrates, and uses chloroform extraction, abandons chloroform layer, and reconcentration to proportion is 1, separates out crystallization for 0-4 ℃.
Crystallization with 50% ethyl alcohol recrystallization, is filtered, drying, crystallization shape powder, to reach the purpose of purification.
Embodiment 6
Extract the technology of phlorizin a kind of skin, root, branches and leaves and the waste material of squeezing the juice, comprise the steps: from rosaceous plant
(1) spray is cut into segment about 1cm, the percent by volume that adds 6 times is 30% ethanol, soaks 2 hours, is heated to and boils, and keeps little and boils 2 hours, filters; Residue is that 30% ethanol is heated to and boils with 2 times percent by volume, keeps little and boils 3 hours, collects filtered liquid, concentrates to reclaim ethanol to filtered liquid and do not have the alcohol flavor; (2) filtered liquid is through macroporous resin adsorption, and the ethanol gradient elution with 20%, 40%, 60%, 80% with the effluent liquid Fractional Collections, concentrates, and uses chloroform extraction, abandons chloroform layer, and reconcentration to proportion is 1, separates out crystallization for 0-4 ℃.
Crystallization with 50% ethyl alcohol recrystallization, is filtered, drying, crystallization shape powder, to reach the purpose of purification.
Embodiment 6
Can be that raw material extracts phlorizin by the step of above-mentioned several embodiment with the bark of rosaceous plant or root and the immature vegetables and fruits in the fruit planting process.
Embodiment 7
Extract the technology of phlorizin a kind of skin of the present invention, root, branches and leaves and the waste material of squeezing the juice from rosaceous plant, the mensuration of the phlorizin that extracts is the HPLC method that adopts, and has obtained Fig. 2, Fig. 3, and Fig. 2 and Fig. 3 compare with standard substance Fig. 4, proof, the content of the phlorizin that the present invention extracts is higher.
Claims (4)
1. extract the technology of phlorizin the skin from rosaceous plant, root, branches and leaves and the waste material of squeezing the juice, its feature comprises the steps: that (1) adds 4-10 percent by volume doubly with raw material is the ethanol of 30%-70%, soaks 1-3 hour, is heated to and boils, keep little and boiled 2-3 hour, filter; Residue is that the ethanol of 30%-70% is heated to and boils with 2-8 percent by volume doubly, keeps little and boiled 2-3 hour, this process 1 to 3 once, collect filtered liquid, concentrate and reclaim ethanol to filtered liquid and do not have alcohol and distinguish the flavor of; (2) filtered liquid is through macroporous resin adsorption, and the ethanol gradient elution with 20%, 40%, 60%, 80% with the effluent liquid Fractional Collections, concentrates, and uses chloroform extraction, abandons chloroform layer, and reconcentration to proportion is 1-1.08, separates out crystallization for 0-4 ℃.
2. extract the technology of phlorizin a kind of skin from rosaceous plant according to claim 1, root, branches and leaves and the waste material, it is characterized in that the ethyl alcohol recrystallization of described crystallization with 40%-60%, filter, drying gets crystallization shape powder.
3. extract the technology of phlorizin a kind of skin according to claim 1, root, branches and leaves and the waste material, it is characterized in that described rosaceous plant is apple or pears or peach or cherry from rosaceous plant.
4. extract the technology of phlorizin a kind of skin from rosaceous plant according to claim 1, root, branches and leaves and the waste material of squeezing the juice, the amount of alcohol that it is characterized in that described immersion raw material is 6-8 a times of raw material.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100162914A CN100463913C (en) | 2005-03-11 | 2005-03-11 | Process for extracting phlorhizin from bark, root, branch and leaf of rosaceous plant and juice pressing waste material |
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| CNB2005100162914A CN100463913C (en) | 2005-03-11 | 2005-03-11 | Process for extracting phlorhizin from bark, root, branch and leaf of rosaceous plant and juice pressing waste material |
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| CN1683382A true CN1683382A (en) | 2005-10-19 |
| CN100463913C CN100463913C (en) | 2009-02-25 |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811949A (en) * | 2010-05-14 | 2010-08-25 | 上海利盛生化有限公司 | Purification method of phloretin powder |
| CN101897776A (en) * | 2009-06-01 | 2010-12-01 | 汪鋆植 | New application of Chinese flowing crabapple extractive and phlorizin |
| CN101006792B (en) * | 2006-12-30 | 2011-05-18 | 三峡大学 | Method for preparing anti-virus medicine of crabapple and its applications |
| CN102086220A (en) * | 2010-12-31 | 2011-06-08 | 广州市天吻娇颜化妆品有限公司 | Extraction and purification method of phlorizin in litchi peels |
| CN101683351B (en) * | 2008-09-24 | 2011-09-07 | 汪鋆植 | Application of phlorizin in preparing hepatic or health-care food |
| CN102697895A (en) * | 2012-06-11 | 2012-10-03 | 陕西师范大学 | Method for continuously extracting total polyphenol, chlorogenic acid and phlorizin from green apples |
| CN104045671A (en) * | 2013-03-16 | 2014-09-17 | 永州一东生物技术有限责任公司 | Method for extracting and purifying phlorizin in apple root-bark |
| CN104610394A (en) * | 2015-01-30 | 2015-05-13 | 望宏端 | Method for extracting phlorizin with different purity from twigs and green leaves of Malus hupehensis |
| CN105777822A (en) * | 2016-04-17 | 2016-07-20 | 中国农业科学院郑州果树研究所 | Method for preparing high-purity phloridzin by virtue of apple tree branches |
| CN105924482A (en) * | 2016-04-29 | 2016-09-07 | 中南林业科技大学 | Method for extracting phloretin from camellia oleifera leaves |
| CN106336441A (en) * | 2015-07-07 | 2017-01-18 | 天津优利果蔬食品有限公司 | Extraction process of high-purity phloridzin |
| CN107722664A (en) * | 2017-09-18 | 2018-02-23 | 炉霍雪域俄色有限责任公司 | A kind of method that uranidin is extracted from Malus toringoides Hughes |
| CN107759645A (en) * | 2017-09-18 | 2018-03-06 | 炉霍雪域俄色有限责任公司 | A kind of method that phloridzin is extracted in the slag from Malus toringoides Hughes |
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| SU1309539A1 (en) * | 1985-04-18 | 1996-04-20 | Плодоовощной институт им.И.В.Мичурина | Process for recovering phlorizin from bark of apple tree sprouts |
| JP3957087B2 (en) * | 1995-05-29 | 2007-08-08 | ニッカウヰスキー株式会社 | Apple red pigment and its production method, antioxidant, antihypertensive agent, allergy inhibitor, anti-cariogenic agent and deodorant |
| JPH09175982A (en) * | 1995-12-28 | 1997-07-08 | Nikka Uisukii Kk | Cosmetic |
| FR2799121B1 (en) * | 1999-10-01 | 2004-02-13 | Fabre Pierre Dermo Cosmetique | EXTRACTS FROM APPLE BRANCHES USEFUL IN DERMOCOSMETOLOGY AND THEIR PREPARATION PROCESS |
| DE10018533C2 (en) * | 2000-04-13 | 2002-10-31 | Herbstreith & Fox Kg Pektin Fa | Process for the recovery of valuable materials from by-products of fruit and vegetable processing |
| FR2822466B1 (en) * | 2001-03-23 | 2004-07-02 | Diana Ingredients | PHLORIDZINE-RICH PHENOLIC FRACTION AND ITS USE AS A COSMETIC, FOOD OR NUTRACEUTICAL AGENT |
| CN1166662C (en) * | 2001-07-25 | 2004-09-15 | 於洪建 | Malic polyphenol producing process with apple peel slag |
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2005
- 2005-03-11 CN CNB2005100162914A patent/CN100463913C/en active Active
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101006792B (en) * | 2006-12-30 | 2011-05-18 | 三峡大学 | Method for preparing anti-virus medicine of crabapple and its applications |
| CN101683351B (en) * | 2008-09-24 | 2011-09-07 | 汪鋆植 | Application of phlorizin in preparing hepatic or health-care food |
| CN101897776A (en) * | 2009-06-01 | 2010-12-01 | 汪鋆植 | New application of Chinese flowing crabapple extractive and phlorizin |
| CN101811949A (en) * | 2010-05-14 | 2010-08-25 | 上海利盛生化有限公司 | Purification method of phloretin powder |
| CN101811949B (en) * | 2010-05-14 | 2013-06-05 | 上海利盛生化有限公司 | Purification method of phloretin powder |
| CN102086220A (en) * | 2010-12-31 | 2011-06-08 | 广州市天吻娇颜化妆品有限公司 | Extraction and purification method of phlorizin in litchi peels |
| CN102697895A (en) * | 2012-06-11 | 2012-10-03 | 陕西师范大学 | Method for continuously extracting total polyphenol, chlorogenic acid and phlorizin from green apples |
| CN102697895B (en) * | 2012-06-11 | 2014-03-05 | 陕西师范大学 | Method for continuously extracting total polyphenol, chlorogenic acid and phlorizin from green apples |
| CN104045671A (en) * | 2013-03-16 | 2014-09-17 | 永州一东生物技术有限责任公司 | Method for extracting and purifying phlorizin in apple root-bark |
| CN104610394A (en) * | 2015-01-30 | 2015-05-13 | 望宏端 | Method for extracting phlorizin with different purity from twigs and green leaves of Malus hupehensis |
| CN106336441A (en) * | 2015-07-07 | 2017-01-18 | 天津优利果蔬食品有限公司 | Extraction process of high-purity phloridzin |
| CN105777822A (en) * | 2016-04-17 | 2016-07-20 | 中国农业科学院郑州果树研究所 | Method for preparing high-purity phloridzin by virtue of apple tree branches |
| CN105777822B (en) * | 2016-04-17 | 2019-07-12 | 中国农业科学院郑州果树研究所 | A method of phloridzin is prepared using apple branch |
| CN105924482A (en) * | 2016-04-29 | 2016-09-07 | 中南林业科技大学 | Method for extracting phloretin from camellia oleifera leaves |
| CN107722664A (en) * | 2017-09-18 | 2018-02-23 | 炉霍雪域俄色有限责任公司 | A kind of method that uranidin is extracted from Malus toringoides Hughes |
| CN107759645A (en) * | 2017-09-18 | 2018-03-06 | 炉霍雪域俄色有限责任公司 | A kind of method that phloridzin is extracted in the slag from Malus toringoides Hughes |
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Denomination of invention: Process for extracting phlorhizin from bark, root, branch and leaf of rosaceous plant and juice pressing waste material Effective date of registration: 20101206 Granted publication date: 20090225 Pledgee: Tianjin TEDA Small Enterprise Credit Guarantee Center Pledgor: Jianfeng Natural Product R&D Development Co., Ltd., Tianjin Registration number: 2010990000991 |
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Date of cancellation: 20110801 Granted publication date: 20090225 Pledgee: Tianjin TEDA Small Enterprise Credit Guarantee Center Pledgor: Jianfeng Natural Product R&D Development Co., Ltd., Tianjin Registration number: 2010990000991 |